原位聚合聚苯胺层层自组装膜的制备及其敏感性能研究
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摘要
层层自组装(LBL-SA)技术是制备敏感薄膜的一种有效手段,该技术成膜物质丰富,可在任何形状和大小的基片上成膜,而且还能精确控制薄膜的厚度与单层膜的结构。本文针对聚苯胺(PANI)难溶难融、聚苯胺敏感膜响应时间长和敏感下限高等缺陷,从苯胺单体(AN)出发,通过原位聚合及现场掺杂,并主要基于静电力、氢键作用LBL-SA制备了具有纳米结构的聚苯胺自组装膜,探讨了该自组装膜的成膜机理,考察了该自组装膜对NH_3的敏感性能;进而调节聚苯胺自组装膜的结构,考察了不同掺杂结构的聚苯胺自组装膜的抗湿性能和对化学战剂模拟剂的敏感性能。
跟踪了原位聚合的具有纳米结构的聚苯胺多层自组装膜的成膜过程,提出了该自组装膜的成膜机理:聚合反应初始阶段的苯胺阳离子或苯胺阳离子自由基通过静电作用快速吸附到带负电荷的基片表面,形成均匀的聚合中心,然后以垂直于基片的方式进行链增长生成PANI;PANI在酸性条件下经现场掺杂后带正电荷,再通过静电作用吸附带负电荷的聚电解质如聚苯乙烯磺酸钠(PSS),或通过氢键作用吸附聚合物如聚乙烯醇(PVA),这样循环LBL-SA即得到(PSS/PANI)_n或(PVA/PANI)_n等原位聚合聚苯胺自组装膜。
在探讨成膜机理的基础上,成功制备了结构与性能可调、稳定、多孔、无定型的(PSS/PANI)_n纳米自组装膜。确定了膜厚为30～100 nm的单个双层PSS/PANI自组装膜的较优制备工艺条件:PSS溶液的浓度为0.001 mol·L~(-1)～0.02 mol·L~(-1)、沉积时间不少于10 min、氧化剂过硫酸铵(APS)以分段滴加的方式加入AN活性溶液中、APS与AN的物质的量之比(n_(APS):n_(An))为0.8～1.2。在此工艺基础上,进一步调节AN浓度,制备了逐层均匀增长、性能较优的多层(PSS/PANI)_n自组装膜。
基于(PSS/PANI)_n自组装膜对NH_3的化学吸附而使膜电阻增大的原理,考察了该自组装膜对氨气的敏感性能,结果表明:该自组装膜对NH_3响应迅速、检测下限低、敏感度高、选择性好。当NH_3的检测浓度为0.1 mg/m~3时,该膜的相对灵敏度可达63.47%,而响应时间仅为39s。这一研究为制备灵敏度高、选择性好的聚苯胺氨气传感器奠定了坚实的理论基础和实验基础。
利用聚苯胺的掺杂特性对PSS/PANI自组装膜进行了结构调节,提高了该膜的抗湿性能。首次考察了不同掺杂/脱掺杂结构的PSS/PANI自组装膜对化学战剂模拟剂DMMP和CEES的敏感性能,研究表明,掺杂酸对离子的尺寸大小对PSS/PANI自组装膜的气敏性有很大影响,较大的对离子尺寸有利于提高自组装膜的气敏性;并且发现采用与DMMP结构类似的沙林酸对EB-PSS/PANI自组装膜进行再掺杂-脱掺杂,能显著提高PSS/PANI自组装膜对DMMP的敏感性能。
拓展了聚苯胺LBL自组装膜的界面构建、新型膜的固定等基础性问题研究。基于氢键作用,通过原位聚合的聚苯胺LBL-SA制备了(PVA/PANI)_n多层自组装膜;从邻甲基苯胺单体(OT)出发原位聚合,再通过静电作用LBL-SA制备了(PSS/POT)_n多层自组装膜。研究表明,可以依据实际需要构建含有PANI、PSS、PVA或POT等多组分的、组装顺序可变的LBL自组装膜,为寻求具有多途径可调结构的聚苯胺自组装膜以提高对化学战剂的敏感性能奠定了基础。
Layer-by-layer self-assembly (LBL-SA) technique is a simple, rapid and effective method to prepare ultra-thin sensitive films. The fabricated films comprise a variety of materials in accordance to the requirement and can be constructed on any shape and size of substrates by different processing parameters. The average thickness and surface function of each monolayer can be accurately controlled and tuned. Polyaniline (PANI) is one of the most potential conductive polymers, but the further applications of polyaniline are restricted by the low solubility and high melting temperature of polyaniline, and long response time and high threshold detection limit of polyaniline films. In this dissertation, we focus on the investigation of polyaniline films that were fabricated from aniline (AN) monomers by in situ polymerization, self-acid-doping and layer-by-layer self-assembly through the electrostatic force or hydrogen bonding. Formation mechanism of the PANI self-assembled films was proposed. The detection of NH3 using as prepared PANI films was also studied. Furthermore, the structure of the PANI films was tuned by acid doping or dedoping. The humidity resistance and the sensitivity to chemical warfare agents (CWAs) simulants of the tuned films were also investigated.
Self-assembled LBL polyaniline films were prepared from aniline monomers by in situ polymerization and the mechanism of film formation was discussed. It was proposed that the self-assembly of polyaniline occurred through the quick absorption of aniline monomer cations or aniline monomer cation radicals on the glass surfaces by electrostatic attractions to form homogeneous polymerization centers, then increased gradually by the way of upright to the glass supports for extensity, leading to the polyaniline chain growth. The polyaniline was doped under acidic condition to absorb anionic polyelectrolyte, such as sodium polystyrene sulfonate (PSS) based on the electrostatic force, or to adsorb polymer based on hydrogen-bonding interactions, for example Polyvinyl Alcohol (PVA), and then recycled to fabricate (PSS/PANI)_n or (PVA/PANI)_n self-assembled multilayer films.
Based on the formation mechanism of the film, stable, porous, and amorphous nano-structured (PSS/PANI)_n multilayer films with adjustable structure and properties were prepared. The deposition conditions for the fabrication of 30 - 100 nm PSS / PANI films were optimized. The optimum deposition conditions are: the concentration of PSS solution is 0.001 - 0.02 mol·L~(-1), the molar ratio of oxidant to aniline (n_(ASPS) : n_(An)) is 0.8 -1.2, the oxidant APS is added into the aniline solution at different polymerization stages, and the deposition time should be at least 10 min. Under this optimum deposition conditions, (PSS/PANI)_n multilayer films with equal thickness of each layer and good conductivity were prepared by adjusting the concentration of aniline solution and the in situ polymerization time.
Based on the principle that resistance of (PSS/PANI)_n self-assembled films increases due to the chemical absorption of NH_3, its sensitivity to NH_3 was investigated. Results show that these films exhibit quick response, low detecting limit, high sensitivity, and good selectivity. When the concentration of NH_3 is 0.1 mg/m~3 , the relative sensitivity of this film is 63.47 % and the response time is only 39 s. This established foundations for the preparation of polyaniline NH_3 sensor with high sensitivity and good selectivity.
The humidity resistance of PSS/PANI self-assembled film was improved by adjusting its structure through redoping. Sensing ability of PSS/PANI self-assembled film with different doping/dedoping structure to DMMP and CEES was investigated. Results demonstrate that the gas sensitivity of PSS/PANI self-assembled film is affected by the size of dopant counterions. Gas sensitivity of self-assembled film increases with increasing size of dopant counterions. It is found that sensing ability of PSS/PANI self-assembled film to DMMP increases significantly by redoping/dedoping EB-PSS/PANI film with sarin acid that has similar structure with DMMP.
Interface construction and preparation of new in situ polymerized polyaniline layer-by-layer self assembled films were also investigated. (PANI/PVA)_n films were prepared from aniline monomers by in situ polymerization, and layer-by-layer self-assembly through the hydrogen bond; (PSS/POT)_n films were prepared from o-methylaniline monomers by in situ polymerization, and layer-by-layer self-assembly through the electronstatic bond. All results suggested that uniform thin composite film containing PANI, PSS, PVA, or POT could be fabricated using this simple process and the order of these polymers could be changed as required. Consequently, it is possible to increase the sensitivity of polyaniline self-assembled film to CWAs through adjusting the structure of the films.
跟踪了原位聚合的具有纳米结构的聚苯胺多层自组装膜的成膜过程,提出了该自组装膜的成膜机理:聚合反应初始阶段的苯胺阳离子或苯胺阳离子自由基通过静电作用快速吸附到带负电荷的基片表面,形成均匀的聚合中心,然后以垂直于基片的方式进行链增长生成PANI;PANI在酸性条件下经现场掺杂后带正电荷,再通过静电作用吸附带负电荷的聚电解质如聚苯乙烯磺酸钠(PSS),或通过氢键作用吸附聚合物如聚乙烯醇(PVA),这样循环LBL-SA即得到(PSS/PANI)_n或(PVA/PANI)_n等原位聚合聚苯胺自组装膜。
在探讨成膜机理的基础上,成功制备了结构与性能可调、稳定、多孔、无定型的(PSS/PANI)_n纳米自组装膜。确定了膜厚为30～100 nm的单个双层PSS/PANI自组装膜的较优制备工艺条件:PSS溶液的浓度为0.001 mol·L~(-1)～0.02 mol·L~(-1)、沉积时间不少于10 min、氧化剂过硫酸铵(APS)以分段滴加的方式加入AN活性溶液中、APS与AN的物质的量之比(n_(APS):n_(An))为0.8～1.2。在此工艺基础上,进一步调节AN浓度,制备了逐层均匀增长、性能较优的多层(PSS/PANI)_n自组装膜。
基于(PSS/PANI)_n自组装膜对NH_3的化学吸附而使膜电阻增大的原理,考察了该自组装膜对氨气的敏感性能,结果表明:该自组装膜对NH_3响应迅速、检测下限低、敏感度高、选择性好。当NH_3的检测浓度为0.1 mg/m~3时,该膜的相对灵敏度可达63.47%,而响应时间仅为39s。这一研究为制备灵敏度高、选择性好的聚苯胺氨气传感器奠定了坚实的理论基础和实验基础。
利用聚苯胺的掺杂特性对PSS/PANI自组装膜进行了结构调节,提高了该膜的抗湿性能。首次考察了不同掺杂/脱掺杂结构的PSS/PANI自组装膜对化学战剂模拟剂DMMP和CEES的敏感性能,研究表明,掺杂酸对离子的尺寸大小对PSS/PANI自组装膜的气敏性有很大影响,较大的对离子尺寸有利于提高自组装膜的气敏性;并且发现采用与DMMP结构类似的沙林酸对EB-PSS/PANI自组装膜进行再掺杂-脱掺杂,能显著提高PSS/PANI自组装膜对DMMP的敏感性能。
拓展了聚苯胺LBL自组装膜的界面构建、新型膜的固定等基础性问题研究。基于氢键作用,通过原位聚合的聚苯胺LBL-SA制备了(PVA/PANI)_n多层自组装膜;从邻甲基苯胺单体(OT)出发原位聚合,再通过静电作用LBL-SA制备了(PSS/POT)_n多层自组装膜。研究表明,可以依据实际需要构建含有PANI、PSS、PVA或POT等多组分的、组装顺序可变的LBL自组装膜,为寻求具有多途径可调结构的聚苯胺自组装膜以提高对化学战剂的敏感性能奠定了基础。
Layer-by-layer self-assembly (LBL-SA) technique is a simple, rapid and effective method to prepare ultra-thin sensitive films. The fabricated films comprise a variety of materials in accordance to the requirement and can be constructed on any shape and size of substrates by different processing parameters. The average thickness and surface function of each monolayer can be accurately controlled and tuned. Polyaniline (PANI) is one of the most potential conductive polymers, but the further applications of polyaniline are restricted by the low solubility and high melting temperature of polyaniline, and long response time and high threshold detection limit of polyaniline films. In this dissertation, we focus on the investigation of polyaniline films that were fabricated from aniline (AN) monomers by in situ polymerization, self-acid-doping and layer-by-layer self-assembly through the electrostatic force or hydrogen bonding. Formation mechanism of the PANI self-assembled films was proposed. The detection of NH3 using as prepared PANI films was also studied. Furthermore, the structure of the PANI films was tuned by acid doping or dedoping. The humidity resistance and the sensitivity to chemical warfare agents (CWAs) simulants of the tuned films were also investigated.
Self-assembled LBL polyaniline films were prepared from aniline monomers by in situ polymerization and the mechanism of film formation was discussed. It was proposed that the self-assembly of polyaniline occurred through the quick absorption of aniline monomer cations or aniline monomer cation radicals on the glass surfaces by electrostatic attractions to form homogeneous polymerization centers, then increased gradually by the way of upright to the glass supports for extensity, leading to the polyaniline chain growth. The polyaniline was doped under acidic condition to absorb anionic polyelectrolyte, such as sodium polystyrene sulfonate (PSS) based on the electrostatic force, or to adsorb polymer based on hydrogen-bonding interactions, for example Polyvinyl Alcohol (PVA), and then recycled to fabricate (PSS/PANI)_n or (PVA/PANI)_n self-assembled multilayer films.
Based on the formation mechanism of the film, stable, porous, and amorphous nano-structured (PSS/PANI)_n multilayer films with adjustable structure and properties were prepared. The deposition conditions for the fabrication of 30 - 100 nm PSS / PANI films were optimized. The optimum deposition conditions are: the concentration of PSS solution is 0.001 - 0.02 mol·L~(-1), the molar ratio of oxidant to aniline (n_(ASPS) : n_(An)) is 0.8 -1.2, the oxidant APS is added into the aniline solution at different polymerization stages, and the deposition time should be at least 10 min. Under this optimum deposition conditions, (PSS/PANI)_n multilayer films with equal thickness of each layer and good conductivity were prepared by adjusting the concentration of aniline solution and the in situ polymerization time.
Based on the principle that resistance of (PSS/PANI)_n self-assembled films increases due to the chemical absorption of NH_3, its sensitivity to NH_3 was investigated. Results show that these films exhibit quick response, low detecting limit, high sensitivity, and good selectivity. When the concentration of NH_3 is 0.1 mg/m~3 , the relative sensitivity of this film is 63.47 % and the response time is only 39 s. This established foundations for the preparation of polyaniline NH_3 sensor with high sensitivity and good selectivity.
The humidity resistance of PSS/PANI self-assembled film was improved by adjusting its structure through redoping. Sensing ability of PSS/PANI self-assembled film with different doping/dedoping structure to DMMP and CEES was investigated. Results demonstrate that the gas sensitivity of PSS/PANI self-assembled film is affected by the size of dopant counterions. Gas sensitivity of self-assembled film increases with increasing size of dopant counterions. It is found that sensing ability of PSS/PANI self-assembled film to DMMP increases significantly by redoping/dedoping EB-PSS/PANI film with sarin acid that has similar structure with DMMP.
Interface construction and preparation of new in situ polymerized polyaniline layer-by-layer self assembled films were also investigated. (PANI/PVA)_n films were prepared from aniline monomers by in situ polymerization, and layer-by-layer self-assembly through the hydrogen bond; (PSS/POT)_n films were prepared from o-methylaniline monomers by in situ polymerization, and layer-by-layer self-assembly through the electronstatic bond. All results suggested that uniform thin composite film containing PANI, PSS, PVA, or POT could be fabricated using this simple process and the order of these polymers could be changed as required. Consequently, it is possible to increase the sensitivity of polyaniline self-assembled film to CWAs through adjusting the structure of the films.
引文
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